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采用高效液相色谱-电感耦合等离子体质谱(HPLC-ICP-MS)联用技术建立了烟草中硒的形态分析方法。烟草样品采用0.10mol/L HCl超声提取30min,经离心、过膜后引入HPLC-ICP-MS进行分析。使用Hamilton PRP X-100阴离子交换柱,以20mmol/L柠檬酸水溶液为流动相(pH=7.0),流速1.2mL/min,优化条件下实现了6种硒形态的分离。质谱采用He碰撞模式,硒代胱氨酸、亚硒酸根、甲基硒代半胱氨酸、硒酸根、硒脲、硒代蛋氨酸检出限分别为1.20、0.34、1.65、0.13、3.25和0.65ng/mL。该方法操作简单、快速、灵敏度高,精密度好,加标回收率在86.1%~95.8%之间,适用于烟草中硒元素形态分析。
The method for speciation analysis of selenium in tobacco has been established by using high performance liquid chromatography-inductively coupled plasma mass spectrometry (HPLC-ICP-MS). Tobacco samples were extracted by sonication with 0.10mol / L HCl for 30min, centrifuged and analyzed by HPLC-ICP-MS. Using Hamilton PRP X-100 anion exchange column, the mobile phase (pH = 7.0) was 20mmol / L citric acid solution and the flow rate was 1.2mL / min. Separation of six selenium forms was achieved under the optimized conditions. The detection limits were 1.20, 0.34, 1.65, 0.13, 3.25 and 0.65 for the mass spectrum using the He collision mode. The detection limits of selenocysteine, selenite, methylselenocysteine, selenate, selenourea and selenomethionine were ng / mL. The method is simple, rapid, sensitive and accurate. The recoveries of spiked samples ranged from 86.1% to 95.8%. It is suitable for speciation analysis of selenium in tobacco.